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1.
Three new amphiphilic compounds i.e., n-decyl-3-methylpyridinium bromide (a), n-dodecyl-3-methylpyridinium bromide (b), and n-tetradecyl-3-methylpyridinium bromide (c), have been synthesized by condensation reaction and characterized by NMR (1H, 13C) and FTIR spectroscopic techniques. The micellization behavior of the compounds has been studied in ethanol employing conductometry and UV/visible spectroscopy. The critical micellization concentration (CMC) values for compound a, b and c was found to be 0.31, 0.29 and 0.27 m mol L?1, respectively. Effect of temperature on the CMC was checked in the range of 298-318 K. The thermodynamic parameters such as ΔG, ΔH and ΔS of the micellization process of these surfactants were computed. The negative values of ΔG and positive values of ΔH indicated the spontaneous and endothermic nature of the micellization process. Antimicrobial activities of these amphiphiles showed significant activity against different bacterial strains.  相似文献   

2.
The naturally occurring (6Z)-(±)-2-methoxy-6-hexadecenoic acid (1) and (6Z)-(±)-2-methoxy-6-octadecenoic acid (2) were synthesized in 7–8 steps with 38 and 13% overall yields, respectively, by using an acetylide coupling approach, which made it possible to obtain a 100% cis-stereochemistry for the double bonds. In a similar fashion, the acetylenic analogs (±)-2-methoxy-6-hexadecynoic acid (3) and (±)-2-methoxy-6-octadecynoic acid (4) were also synthesized in 6–7 steps with 48 and 16% overall yields, respectively. The antibacterial activity of acids 14 was determined against clinical isolates of methicillin-resistant Staphylococcus aureus (ClMRSA) and Escherichia coli. Among the series of compounds, acid 4 was the most active bactericide towards CIMRSA displaying IC50s (half maximal inhibitory concentrations) between 17 and 37 μg/mL, in sharp contrast to the 6-octadecynoic acid, which was not bactericidal at all. On the other hand, acids 1 and 3 were the only acids that displayed antibacterial activity towards E. coli, but 1 stood out as the best candidate with an IC50 of 21 μg/mL. The critical micelle concentrations (CMCs) of acids 14 were also determined. The C18 acids 2 and 4 displayed a five-fold lower CMC (15–20 μg/mL) than the C16 analogs 1 and 3 (70–100 μg/mL), indicating that 4 exerts its antibacterial activity in a micellar state. None of the studied acids were inhibitory towards S. aureus DNA gyrase discounting this type of enzyme inhibition as a possible antibacterial mechanism. It was concluded that the combination of α-methoxylation and C-6 unsaturation increases the bactericidal activity of the C16 and C18 FA towards the studied bacterial strains. Acids 1 and 4 stand out as viable candidates to be used against E. coli and CIMRSA, respectively.  相似文献   

3.
Three new metal(II) complexes based on N-methylimidazole, [ML6]·(SH)2·(H2O)2, (M = Ni(II) (1), Co(II) (2), Cu(II) (3), L=N-methylimidazole), have been synthesized and characterized. The single crystal X-ray structural analyses show that complexes 1, 2, and 3 have isomorphous structures and crystallize in monoclinic system with space group P21/c. The complexes containing isolated SH? anions, which may come from the thermochemical sulfate reduction, are located in the gap with lattice water molecules and provide multiple intermolecular hydrogen bonds to form 2D layers. Topology analyses show a 2D hydrogen bond network, which can be regarded as an unprecedented trinodal (3,4,6)-connected topology with Schläfli symbol (3.4.53.6)2(3.4.5)2(32;54;64;82;93). Cyclic voltammetry and UV–vis spectra were studied.  相似文献   

4.
Octa(aminophenyl)-T8-polyhedral silsesquioxane, 1, can serve as a cross-linking agent for organic polymeric resins. Amino functional groups of 1 can form chemical bonds or hydrogen-bonds to appropriate matrix polymers or resins. Various resole phenolic resin/1 nanocomposites (0, 1, 3, 6, and 12 wt% 1) were prepared. Hydrogen bonding between phenolic hydroxyls and the amino groups of 1 in these nanocomposites were investigated by FT-IR. The aggregation morphologies of 1 within these samples were examined using SEM, TEM, and Wide Angle X-ray Diffraction (WAXD) studies. Small quasispherical nanometer-sized POSS particles which were further aggregated into clusters, like individual grapes in a bunch, formed into phase-separated domains as large as 400 nm in diameter as the loading of 1 increased. These particles exhibited a broad 2θ = 5.8° WAXD peak indicating the presence of some crystalline order within the nanoparticles of 1 making up the aggregates. This corresponds to an average crystalline plane lattice distance of 17.5 Å. However, extraction of the finely powdered nanocomposites by refluxing THF failed to remove 1 indicating the vast majority of 1 must be chemically bound. Thus, the aggregates must have resin within their structure. The storage modulus (E') in both the glassy and rubbery regions, thermal stability, and glass transition temperature of the composites were improved by 1 wt% 1. However, at high loadings of 1, these properties gradually decreased. Surface extractions by THF removed only a portion of the 1 in the surface regions based on X-EDS analyses for Si, suggesting that a portion of 1 might chemically bond into the phenolic resin matrix during the cure. As the loading of 1 increased, the content of 1 at specific surface locations gradually tends to increase and confirmed excellent dispersion of 1 in the micron size-scale at all locations.  相似文献   

5.
[Co2(L1)2(NCS)4]·4MeOH 1, [Co(L2)2(H2O)2](Sal)2·4H2O (Sal = salicylate) 2 were obtained from self-assembly of the cobalt salts with bis(N-benzimidazolyl)methane (L1), and bis(N-benzimidazolyl)methane (L2), and their structures were characterized by IR and X-ray diffraction analysis. Complex 1 exhibits a two-dimensional grid structure, whereas complex 2 is a coordination polymer having a one-dimensional linear chain structure. The grid in 1 lies parallel to the crystallographic ab plane and exhibits intra-grid M–M separations of 10.508 × 10.508 Å. Hydrogen bonds hold the cationic chains in 2 together leading to a three-dimensional network structure.  相似文献   

6.
A cathode material for lithium-ion batteries–LiNi1/3Co1/3Mn1/3O2–was prepared by solution combustion synthesis and characterized by XRD, SEM, and galvanostatic charge/discharge cycling. The sample calcined at 950°C for 10 h showed best charge/discharge performance. An initial discharge capacity (C) of 150.5 mA h g–1 retained 95.7% of its value after 75 charge/discharge cycles at Ic = 14 mA g–1 (0.2C rate), Id = 70 mA g–1 (0.5C rate).  相似文献   

7.
Ce1?x Cu x O2 oxide solid solution catalysts with different Ce/Cu mole ratios were synthesized by the one-pot complex method. The prepared Ce1?x Cu x O2 catalysts were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and H2 temperature-programmed reduction (H2-TPR). Their catalytic properties were also investigated by catalytic combustion of phenyl volatile organic compounds (PVOCs: benzene, toluene, xylene, and ethylbenzene) in air. XRD analysis confirmed that the CuO species can fully dissolve into the CeO2 lattice to form CeCu oxide solid solutions. XPS and H2-TPR results indicated that the prepared Ce1?x Cu x O2 catalysts contain abundant reactive oxygen species and superior reducibility. Furthermore, the physicochemical properties of the prepared Ce1?x Cu x O2 catalysts are affected by the Ce/Cu mole ratio. The CeCu3 catalyst with Ce/Cu mole ratio of 3.0 contains abundant reactive oxygen species and exhibits superior catalytic combustion activity of PVOCs. Moreover, the ignitability of PVOCs is also affected by the respective physicochemical properties. The catalytic combustion conversions of ethylbenzene, xylene, toluene, and benzene are 99%, 98.9%, 94.3%, and 62.8% at 205, 220, 225, and 225 °C, respectively.  相似文献   

8.
Anhydrous ammonium pentaborate NH4B5O8 has been synthesized by thermal dehydration of larderellite NH4[B5O7(OH)2] · H2O at a temperature of 290°C for 7 h. The crystal structure has been determined from the X-ray powder diffraction data: a = 7.58667(5) Å, b = 12.00354(8) Å, c = 14.71199(8) Å, R p = 6.23, R wp = 7.98, R B = 12.7, R F = 8.95, and β-KB5O8 structure type. The double interpenetrating framework is formed by pentaborate groups, each consisting of a boron-oxygen tetrahedron and four triangles, in which all oxygen atoms are bridging. The thermal behavior of the NH4B5O8 compound has been investigated using thermal X-ray diffraction. As for other pentaborates of this type, the thermal expansion of the NH4B5O8 compound is anisotropic and reaches a maximum along the a axis. The thermal expansion coefficients are as follows: α a = 39 × 10?6, α b = 6 × 10?6, α c = 20 × 10?6, and α V = 65 × 10?6 °C?1.  相似文献   

9.
It is difficult to research on the surface structure of amorphous phase in fly ash during leaching reaction due to crystalline phase and complex structure. In the present work, in order to reveal the effects of leaching reaction on the surface structure of amorphous phase in fly ash, the modelling CaO-Fe2O3-Al2O3-SiO2 glass was prepared by the traditional melting methods. The leaching reaction of CaO-Fe2O3-Al2O3-SiO2 glass with 7.5 M KOH was investigated by spectroscopy, spectrophotometer and wet chemical method. The results show that the content of Q 1, Q 2, Q 3 and Q 4 of glass without corrosion was 4.21, 9.51, 23.03 and 52.55%, respectively, which shows that the network polymerization of glass is compact. The leaching reaction of glass can be described by the following equation: dS/dt = k/(r + S 0). Leaching in KOH for various times induces the content of Q 4 and Q 1 to be decreased, and Q 2 and Q 3 increased, resulted in the depolymerization of network and the surface glass dissolved in alkaline solution to form a gel phase. In stage one of leaching reaction, the rate of iron ion leached from glass surface was slow, which resulted in the small slope of straight-line relationship of leaching curve. In the following stage, the leaching rate of iron ion increased with the prolongation of time.  相似文献   

10.
The crystal structure of Pb6O[(Si6Al2)O20)] is investigated using X-ray diffraction. The compound has tetragonal symmetry, space group I4/mmm, a = 11.7162(10) Å, c = 8.0435(12) Å, and V = 1104.13(2) Å3. The structure is refined to R 1 = 0.036 for 562 unique reflections with [F 0] ≥ 4σF. The structure contains two symmetrically independent positions of the Pb2+ cations coordinated by five O atoms (Pb2+-O2? = 2.34–2.68 Å). The TO4 tetrahedra (T = Si, Al) form tubular [(Si6Al2)O20] chains extended along the c axis. The O4 oxygen atom is not bonded to the Si and Al atoms and is octahedrally coordinated by six Pb atoms with the formation of an oxo-centered OPb6 octahedron. The assumption is made that, in some of lead silicate and aluminosilicate glasses, a number of oxygen atoms are located outside the tetrahedral structure and represent segregation centers of the Pb2+ cations due to the formation of oxo-centered complexes.  相似文献   

11.
Atom transfer radical polymerizations (ATRP) of styrene (St) and methyl methacrylate (MMA) mediated by [RuCl2(PPh3)2(amine)] complexes, with amine = pyrrolidine (1), piperidine (2), or perhydroazepine (3), were investigated as a function of time, temperature, and concentrations of monomers and 2-bromoisobutyrate as initiator. The plots of ln([M]0/[M]) vs. time and molecular weights vs. monomer conversion were linear and the dispersity indexes decreased with increasing monomer conversions. The complexes 1, 2, and 3 were able to mediate the polymerizations with acceptable rate and level of control. Differences in the rate and control of polymerization were observed in the order 3 > 2 > 1 for both monomers. The activities were discussed considering the steric hindrance and electronic characteristics of the amines as ancillary ligands in the metal centres, considering studies by cyclic voltammetry and NMR.  相似文献   

12.
The reactions of K3[Cu(CN)4], Me3SnCl and methylpyrazine (Me-pyz) or tetramethylpyrazine (Me4-pyz) in water/dioxane system afforded two new coordination polymers (CP); [{Cu(μ-CN)}2(μ-Me4-pyz)·dioxane] n , 1, and [Cu{μ-Mepyz}{μ-CNSn(Me3)NC–}], 2. X-ray single crystal analysis shows that 1 contains two crystallographically different copper(I) ions which acquire trigonal planar geometry. The structure of 1 contains non-linear (CuCN) chains that are interconnected by the Me4-pyz ligands forming 3D-network structure. The structure of 1 has two-fold interpenetrating 3D-networks with dioxane molecules encapsulated in the voids of the structure. The structures of these CP were also investigated by FTIR and mass spectroscopy, thermal analysis and compared with the prototype compounds. Spectroscopic analyses of 2 confirm the presence of all components (Me3Sn+, Cu(CN)2 ? and Me-pyz) and support the composition predicted by elemental analysis. 1 and 2 display strong fluorescence in the solid state at room temperature.  相似文献   

13.
An aqueous solution of diallylammonium salts (CH2 = CHCH2)2NH+(CH2)3A? having A? as: CO2 ? (I), PO3H2 Cl? (II) and SO3 ? (III) in 1:1:1 mol ratio underwent ammonium persulfate-initiated ter cyclopolymerization to yield pH-responsive zwitterionic polymer IV with random placements of the monomers in the same ratio. During dialysis, PO3H2Cl? of the incorporated monomer units of II upon depletion of HCl became PO3H?. Likewise, azobisisobutyronitrile-initiated cyclopolymerization of I, II, III, and SO2 in a mole ratio of 1:1:1:3 provided pH-responsive tetrapolymer V in over 90 % yield with random and alternative placements of I–III and SO2 units, respectively, in the same ratio as the feed. Polyzwitterions (PZs) IV and V were insoluble in salt-free water but soluble in the presence of salts. The critical salt concentrations required to promote water solubility of PZ IV were determined to be 0.356 M NaCl, 0.237 M NaBr and 0.128 M NaI, whereas for PZ V the corresponding values were found to be 2.25, 1.26 and 0.862 M, respectively. PZs IV and V were converted into anionic polyelectrolytes VI and VII upon basification with NaOH. The viscosity and antiscalant behaviors of VI and VII were examined. The polymers demonstrated remarkable scale inhibition efficacies; at a dose of 10 ppm, both IV (+NaOH) and V (+NaOH) delayed the precipitation of CaSO4 from its supersaturated solution up to 920 and over 4000 min, respectively. For a small concentration of 5 ppm of polymer V, a scale inhibition of 100 % over 100 min verified it to be a potential effective antiscalant additive in reverse osmosis plants.  相似文献   

14.
Two Zn(II) coordination polymers, formulated as {[Zn(L1)0.5(btc)0.5(H2O)]·H2O} n (1) and {[Zn(L2)(1,4-ndc)]·2H2O} n (2) [L1 = 1,4-bis(2-methylbenzimidazole-1-ylmethyl)benzene, L2 = 1,4-bis(2-methylbenzimidazole)butane, H4btc = butane-1,2,3,4-tetracarboxylic acid, 1,4-H2ndc = 1,4-naphthalenedicarboxylic acid] have been synthesized and structurally characterized by single crystal X-ray diffraction. Complex 1 features a 3D (3,4)-connected network with the topology of fsh-3,4-P21/c. Complex 2 is a 2D (4,4) grid with sql topology and further extends into a 3D supramolecular framework by ππ stacking interactions. In addition, the thermal stability, fluorescence, and catalytic properties of two complexes for degrading methyl orange dye in a Fenton-like process were investigated.  相似文献   

15.
Three supramolecular coordination polymers, namely [Ni(L1)(DCTP)(H2O)] n (1), [Cu(L2)(DCTP)] n (2), [Co(L3)(DCTP)] n (3) (L1?=?1,5-bis(5,6-dimethylbenzimidazole)pentane, L2?=?1,4-bis(5,6-dimethylbenzimidazole)butane, L3?=?1,4-bis(benzimidazole)-2-butylene) have been hydrothermally synthesized and characterized by single crystal X-ray structure determination, FT-IR, elemental analysis, X-ray powder diffraction (XPD), and thermogravimetric analysis (TGA). CP 1 exhibits 2D 63 honeycombed network structure, which is further extended into a 3D Moganite (mog) supramolecular framework by classical O–H?O hydrogen-bonding interaction. CPs 2 –3 present 2D (4,4) layers, and 3D supramolecular frameworks that are formed by ππ stacking interactions. Furthermore, the catalytic activities of CPs 1–3 for the degradation of methyl orange in a Fenton-like process has been investigated, and CPs 1–3 show strong photoluminescence properties at room temperature in solid state.  相似文献   

16.
Explored was the influence of compacting pressure (P) and green density (ρ) on the properties of Zr-doped mineral-like pyrochlore ceramics Y2(Ti1 – x Zr x )2O7 (x ≤ 0.3) prepared by SHS method. The optimal ρ values that provide minimal porosity and maximal mechanical strength of synthesized ceramics were found. An increase in ρ was found to decrease combustion temperature and increase pyrochlore lattice parameter a. Green density was also found to affect phase composition of the SHS-produced ceramics under study.  相似文献   

17.
A new compound, CdPb2O2Cl2, is synthesized by the method of solid-phase reactions. The compound has monoclinic symmetry, space group C2/m, a = 12.392(8) Å, b = 3.8040(14) Å, c = 7.658(5) Å, β = 122.64(5)°, and V = 304.0(3) Å3. The structure contains one symmetrically independent position of the Pb2+ cation coordinated by three O2? anions (Pb2+-O2? = 2.29–2.34 Å) and five Cl? anions (Pb2+-Cl? = 3.35–3.57 Å). The Cd2+ cation has a symmetric coordination with the formation of two bonds Cd-O = 2.15 Å and four bonds Cd-Cl = 2.73 Å. The oxygen atom is tetrahedrally coordinated by three Pb2+ cations and one Cd2+ cation, which leads to the formation of oxo-centered heterometallic OPb3Cd tetrahedra. The tetrahedra are linked together into chains through common Pb atoms and into layered complexes due to sharing of the equatorial Cd atoms. The chlorine atoms are located above the cavities of the oxo-centered layer.  相似文献   

18.
Many uncommon non-methylene-interrupted fatty acids (NMI FA) are present in limpet gonads, but their biological properties remain unknown. To investigate new biological effects of naturally occurring NMI FA in eukaryotic cells, the biological activities of structurally analogous (4Z,15Z)-octadecadienoic acid (1), (9Z,20Z)-tricosadienoic acid (2), and (12Z,23Z)-hexacosadienoic acid (3) were examined by using a yeast-based drug-screening system using the Ca2+-sensitive mutant strain, Saccharomyces cerevisiae (zdsergpdrpdr3Δ). Among 13, 1 showed restored growth activity at a dose of 80 µg/disc in the mutant yeast strain. This phenotype suggests that 1 suppresses Ca2+-signaling of the mutant yeast through inhibition of glycogen synthase kinase-3β (GSK-3β) or calcineurin pathways or both. From this result, the inhibitory activity of 13 against GSK-3β was further determined. 13 showed potent inhibitory activity against GSK-3β with IC50 values ranging from 8.7 to 21.9 µM. Inhibition of GSK-3β reduces gene expression of the gluconeogenic key enzymes in liver, so we analyzed glucose production in rat hepatoma H4IIE cells to assess GSK-3β inhibitory activity of 13. Acid 1 inhibited glucose production at 25 µM in H4IIE cells. Our results would open up new possibilities for an anti-diabetic effect of 1 and might provide important insights into understanding the biological properties of naturally occurring NMI FA.  相似文献   

19.
A mononuclear Co(II) derivative, (1) is afforded by employing a ‘scorpionate’ type precursor, bdtbpza [bdtbpza?=?bis(3,5-di-t-butylpyrazol-1-yl)acetate]. Single crystal X-ray structure reveals that the CoII ion exhibits an octahedral geometry possessing on a O6 coordination environment. Detailed EPR interpretation and electrocatalytic hydrogen evolution study are reported. Electrochemical and catalytic study of 1 in DMSO with the presence of acetic acid as weak proton source shows an observed rate constant of 3.7?×?103 s?1 and hydrogen evolution Faradaic efficiency of 74.7%. The catalytic process requires two-electron reduction of the catalyst and formation of a cobalt(II)-hydride species as reactive intermediate.

Graphical Abstract

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20.
New halogenated silicon-containing poly(amides) (PAs) derived from diacids and an aromatic diamine containing an Si atom were obtained according to the Yamazaki procedure. The diacids contain a preformed halogenated imide ring, another amide group and an aminoacidic residue. The diacids and the PAs were characterized by IR and 1H, 13C and 29Si NMR spectroscopy, elemental analysis and, when corresponding, optical rotation. For those PAs containing F atoms in the imide ring, we also observed the signals corresponding to the coupling of the C–F atoms in the 13C MNR spectra. The results are in agreement with the proposed structures. Also, PAs without amino acid residues were synthesized according to the same procedure. PAs were soluble in aprotic polar solvents and some of them in m-cresol and THF, due to the inclusion in the structure of meta-substitution aromatic rings, flexible aminoacidic residue and polar C–Si bonds. The η inh values were low, indicating the presence of oligomeric species of low molecular weight. The T g values did not show a clear tendency about the influence of the nature of the amino acid residue, but when the influence of the halogen atoms was analyzed, it was possible to observe a decrease in the T g values, due to the higher chain separation, and consequently the lower interactions between them. The thermal decomposition temperatures were determined at 10 % of weight loss, showing in general good values between 300 and 367 °C, and not showing a relationship between the values and the structure of the side groups. The transparency was studied observing moderate values at 400 nm, but showing 80 % of transparency between 500 and 550 nm, which was attributed to the higher aromatic content of these PAs. All PAs showed flame retardancy due to the presence of the halogen atoms.  相似文献   

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